인/실리콘 함유 난연성 에폭시 수지의 제조 및 물성

국문 초록 (Abstract)

영구적 난연성기를 함유한 에폭시 수지를 얻기 위하여, 본 연구에서는 디하이드록시를 함유한 인 화합물[10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-oxa-10-phospha phenanthrene-10-oxide, DOPO-HQ]과 디하이드록시를 함유한 실리콘 화합물(polydimethylsiloxane, hydroxyl terminated, PDMS)를 경화하지 않은 에폭시 프리폴리머(diglycidyl ether of bisphenol A, DGEBA)와 반응시킨 다음, 경화제(4,4-diaminodiphenylmethane, DDM)를 사용하여 경화반응 시킨 에폭시 수지를 제조하였다. 제조된 에폭시 수지의 각종 특성을 적외선 분광분석기(FTIR), 시차주사열량기(DSC), 열중량 분석기(TGA), 한계산소지수(LOI)/수직 연소 시험(UL94-V test), 인장 및 충격 시험을 이용하여 분석하였다. 그리고 사용한 인 및 실리콘 화합물의 함량이 에폭시 경화물의 열적/기계적 성질 및 난연성에 미치는 영향을 조사하였다. 인 및 실리콘 성분이 함유된 에폭시 수지의 열적 및 기계적 물성이 단순 에폭시 수지의 물성에 비교하여 크게 향상되었다는 것을 알 수 있었다. 그리고 인 및 실리콘을 함유한 모든 에폭시 수지는 29.9 ~ 31.8%의 LOI 및 V-0 수준의 UL 94-V로 난연성 기준(LOI: 30% 이상, UL 94-V: V-0)을 통과한 반면, 단순 에폭시 수지는 LOI: 21.4% 및 UL 94-V: no rating으로 난연성 기준에 크게 못 미치는 것을 알 수 있었다.

다국어 초록 (Multilingual Abstract)

To obtain epoxy resin with permanently attached flame-retardant groups, phosphorus compound containing di-hydroxyl group [10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-oxa-10-phospha phenanthrene-10-oxide, DOPO-HQ] and silicone compound containing di-hydroxyl group (polydimethylsiloxane, hydroxyl terminated, PDMS) were reacted with uncured epoxy prepolymer (diglycidyl ether of bisphenol A, DGEBA) and then cured using 4,4-diaminodiphenylmethane (DDM) as a crosslinking agent. The properties of the resulting epoxy materials were characterized using Fourier transform infrared (FTIR) spectrometer, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), limiting oxygen index (LOI) test/vertical burning test (UL 94-V test), tensile properties test and impact test. This study examined the effect of phosphorus/silicone compound contents on the thermal/mechanical properties and flame retardancy of cured epoxy resins containing phosphorus and silicone compounds. It was found that the thermal/mechanical properties of epoxy resins containing phosphorus and silicone components were higher than those of simple epoxy resin. The flame-retardancy (LOI: 29.9 ~ 31.8% and UL 94-V: V-0) of all samples containing phosphorus compound and phosphrous compound/silicone compound was found to be passed the flame-retardant requirements (LOI: > 30%, UL 94-V: V-0) of LOI and vertical burning tests. However, the flame-retardancy (LOI: 21.4% and UL 94-V: no rating) of simple epoxy resin was found to be failed the flame-retardant requirements.

목차 (Table of Contents)

• 요약
• Abstract
• 1. 서론
• 2. 실험방법
• 3. 결과 및 고찰
• 4. 결론
• References

참고문헌 (Reference)

1 Wan, I. Y, "Triarylphosphine Oxide Containing Nylon 6,6 Copolymers" American Chemical Society 29-40, 1995

2 Lee, Y. H, "Synthesis and Properties of Waterborne Poly(urethane urea)s Containing Polydimethylsiloxane" 120 : 212-219, 2011

3 Jang, B. N, "Research Trends of Flame Retardant and Flame Retardant Resin" 20 : 8-15, 2009

4 Rakotomalala, M, "Recent Developments in Halogen Free Flame Retardants for Epoxy Resins for Electrical and Electronic Applications" 3 : 4300-4327, 2010

5 Wang, D. Z, "Production and Application of Epoxy Resin" Chemical Industry Press 2001

6 Friedman, R, "Principles of Fire Protection Chemistry and Physics" NFPA 1998

7 Wu, C. S, "Maleimide-epoxy Resins: Preparation, Thermal Properties, and Flame Retardance" 44 : 565-573, 2002

8 Gonzalez, M. G, "Infrared Spectroscopy-Materials Science, Engineering and Technology" InTech 2012

9 Lee, H, "Handbook of Epoxy Resins" McGraw-Hill 1967

10 Hilado, C. J, "Flammability Handbook for Plastics" Technomic publishing 1982

11 Kim, S. J, "Flame Retardant Plastics" 6 : 118-127, 1995

12 Dufton, P. W, "Fire-Additives and Materials" RAPRA Technology LTD 1995

13 May, C. A, "Epoxy Resins Chemistry and Technology" Marcel Dekker 1988

14 Finch, C. A, "Encyclopedia of Polymer Science and Engineering" John Wiley & Sons 7-, 1987

15 Nakamura, Y, "Effects of Particle Size on Mechanical and Impact Properties of Epoxy Resin Filled with Spherical Silica" 45 : 1281-1289, 1992

16 Xiong,, "Development of a DOPO-Containing Melamine Epoxy Hardeners and Its Thermal and Flame-Retardant Properties of Cured Products" 127 : 4352-4358, 2013

17 Smith, C. D, "Department of Chemistry and National Science Foundation Science and Technology Center: High Performance Polymeric Adhesive and Composites" 35 : 108-, 1990

18 Siddaramaiah, J. K. S, "Cure Kinetics of Epoxy Formulations with Diaminodiphenyl Methane" 3 : 114-, 1996

19 Knauss, D. M, "Copolycarbonates and Poly(acrylates) Derived from Hydrolytically Stable Phosphine Oxide Comonomers" American Chemical Society 41-55, 1995

20 Derouet, D, "Chemical Modification of Epoxy Resins by Dialkyl(or aryl) Phosphates:Evaluation of Fire Behavior and Thermal Stability" 62 : 1855-1868, 1996

21 Hill, D. J. T, "A Systematic Study of the Microwave and Thermal Cure Kinetics of the DGEMA/DDA and DGEBA/DDM Epoxy-amine Resin Systems" 13 : 353-, 2002

22 de Miranda, M. I. G, "A D.S.C. Kinetics Study on the Effect of Filler Concentration on Crosslinking of Diglycidylether of Bisphenol-A with 4, 4’-diaminodiphenylmethane" 38 : 1017-, 1997